C
14H
10Cl
2NNaO
2·H
2O
336.15
Benzoic acid,2-[(2,6-dichloro-3-methylphenyl)amino]-,monosodium salt,monohydrate.
Monosodium N-(2,6-dichloro-m-tolyl)anthranilate monohydrate
[6385-02-0].
Anhydrous
318.13
Packaging and storage
Preserve in tight,light-resistant containers.
Identification
A:
Infrared Absorption á197Kñ.
B:
Ultraviolet Absorption 1á197Uñ
Solution:
25µg per mL.
Medium:
0.01Nhydrochloric acid in methanol.
Absorptivities at 242nm,279nm,and 336nm,calculated on the anhydrous basis,do not differ by more than 3.0%.
C:
Ultraviolet Absorption 2á197Uñ
Solution:
1in 40,000.
Medium:
0.1Nsodium hydroxide.
Absorptivities at 279nm and 317nm,calculated on the anhydrous basis,do not differ by more than 3.0%.
Copper
Standard copper solution
Dissolve 1000mg of copper wire in 6mLof nitric acid in a 1Lvolumetric flask.Add 8mLof hydrochloric acid,dilute with water to volume,and mix.Dilute this solution quantitatively and stepwise with water to obtain a Standard copper solutionhaving a known concentration of 0.6µg per mL.
Test solution
Transfer 2g of Meclofenamate Sodium,accurately weighed,to a 100-mLvolumetric flask,and add 1drop of ammonium hydroxide.Dissolve in water,dilute with water to volume,and mix.
Procedure
Concomitantly determine the absorbances of the
Standard copper solutionand the
Test solutionat the copper emission line at about 325nm,with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-scattering á851ñ)equipped with a copper hollow-cathode lamp,using water as the blank.Adjust the operating conditions to obtain about 70%full-scale detector response with the
Standard copper solution.The detector response obtained with the
Test solutionis not greater than that obtained with the
Standard copper solution(0.003%).
Chromatographic purity
Standard solutions
Dissolve an accurately weighed quantity of
USP Meclofenamate Sodium RSin methanol to obtain a solution containing 20mg per mL(
Standard solution A).Dilute 1.0mLof
Standard solution Awith sufficient methanol to obtain 200mLof solution (
Standard solution B).
Test solution
Dissolve 200mg of Meclofenamate Sodium in 10.0mLof methanol.
Procedure
Apply 10-µLportions of
Standard solution A,
Standard solution B,and the
Test solutionto a suitable thin-layer chromatographic plate (see
Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture.Allow the spots to dry,and develop the chromatogram in a solvent system consisting of a mixture of methylene chloride,methyl ethyl ketone,and glacial acetic acid (50:48:2)until the solvent front has moved about eight-tenths of the length of the plate.Remove the plate from the developing chamber,mark the solvent front,and allow the solvent to evaporate.Examine the plate under short-wavelength UVlight:the chromatograms show a principal spot at about the same
RFvalue,and any secondary spot,if present in the chromatogram from the
Test solutionis not more intense than the principal spot obtained from
Standard solution B(0.5%).
Organic volatile impurities,Method Iá467ñ:
meets the requirements.
Assay
Transfer about 350mg of Meclofenamate Sodium,accurately weighed,to a 125-mLseparator,add 10mLof water,and mix to dissolve.To this solution add 3mLof 3Nhydrochloric acid,shake,and extract with three 30-mLportions of chloroform,collecting the chloroform extracts in an evaporating flask.Evaporate the chloroform extracts to dryness.Dissolve the residue in 5mLof dimethyl sulfoxide and 25mLof methanol.Mix,add 5drops of phenolphthalein TS,and titrate the mixture with 0.1Nsodium hydroxide VS.Each mLof 0.1Nsodium hydroxide is equivalent to 31.81mg of C14H10Cl2NNaO2.